Analytic high-speed countercurrent chromatography (HSCCC) was successfully applied to separations of various natural products which include flavonoids from sea buckthorn, alkaloids from Stephania tetrandra S. Moore, hydroxyanthraquinone derivatives from rheum, etc. The results indicated: 1. Efficient separations of multiple components present in a crude extract can be effected in a short period of time by using the normal and reversed elution modes in succession without interrupting the centrifuge run. 2. With chloroform solvent systems, which provide a large difference in density between the two phases, the flow rate can be increased up to 5 ml/min without affecting peak resolution, thus achieving efficient separations in less than 15 minutes as in analytical HPLC. 3. In analogy to the LC/MS system, HSCCC can be effectively interfaced with a mass spectrometer using a thermospray capillary tube device.